CN104583452A - Cylindrical indium sputtering target and process for producing same - Google Patents

Cylindrical indium sputtering target and process for producing same Download PDF

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Publication number
CN104583452A
CN104583452A CN201380044395.9A CN201380044395A CN104583452A CN 104583452 A CN104583452 A CN 104583452A CN 201380044395 A CN201380044395 A CN 201380044395A CN 104583452 A CN104583452 A CN 104583452A
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CN
China
Prior art keywords
indium
cartridge type
target
crystal grain
rounding cartridge
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Granted
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CN201380044395.9A
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Chinese (zh)
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CN104583452B (en
Inventor
远藤瑶辅
铃木秀幸
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JX Nippon Mining and Metals Corp
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JX Nippon Mining and Metals Corp
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/46—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling metal immediately subsequent to continuous casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/002—Hybrid process, e.g. forging following casting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/3423—Shape
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/3426—Material

Abstract

Provided are a cylindrical indium sputtering target which gives a film having a satisfactory thickness distribution and a process for producing the target. In the cylindrical indium target, the entire surface to be sputtered has an average crystal-grain diameter of 1-20 mm. The process for producing a cylindrical indium target comprises a step in which a cylindrical indium target semi-finished product integrated with a backing tube is produced by casting and a step in which the semi-finished product is subjected, throughout the whole length thereof, to radial-direction plastic working at a total draft of 10% or higher.

Description

Indium rounding cartridge type sputtering target and manufacture method thereof
Technical field
The present invention relates to indium rounding cartridge type sputtering target and manufacture method thereof.
Background technology
The sputter target material that indium is formed as the light absorbing zone of Cu-In-Ga-Se system (CIGS) thin-film solar cells uses.
Indium sputtering target manufactures mainly through melting casting, and also there will be a known several relative documents.Such as, in No. 63-44820, Japanese Patent Publication (patent documentation 1), record the manufacture method of following plate sputtering target, after supporting plate is formed indium film, indium is watered and casts from this film and make it to form as one with supporting plate.
On the other hand, in recent years, because the utilising efficiency of target is high, develop so use round tube type sputtering target to replace plate sputtering target.Round tube type sputtering target is forming as fixing target around the support tube (BT) of core, and it can rotate and sputter.Therefore, the whole surface of target becomes degrades region, and is sputtered equably, so can obtain the high utilising efficiency of target.
Even if as the manufacture method of round tube type sputtering target, melting casting is also main flow.In U.S. Patent Application Publication No. 2003/0089482 specification sheets (patent documentation 2), such as record technique as follows.Be that first material of more than 900K forms interior pipe (target support) with fusing point, then, to configure cylindric mould with surrounding the mode coaxial of this interior pipe, and be second material of below 800K is poured into mould and interior pipe gap with molten state by fusing point.When removing mould after cooling curing, the outer tube (target) formed by the second material can be obtained.
In addition, also there will be a known to improve both bonding forces and configure key coat between support tube (BT) and target.Such as in Japanese Unexamined Patent Application Publication 2008-523251 publication (patent documentation 3), record following content: possessing stay pipe and being configured in the tubular target of at least one the target pipe on the periphery of this stay pipe, will there is electroconductibility and the key coat with the wettability being greater than 90% is configured between target pipe and stay pipe.
Prior art document
Patent documentation
Patent documentation 1: Japanese Patent Publication 63-44820 publication
Patent documentation 2: U.S. Patent Application Publication No. 2003/0089482 specification sheets
Patent documentation 3: Japanese Unexamined Patent Application Publication 2008-523251 publication
Summary of the invention
Invent problem to be solved
Like this, round tube type sputtering target is promising technology, but present situation is, insufficient for the research of indium rounding cartridge type sputtering target.Such as, when using melting casting to manufacture indium rounding cartridge type sputtering target, the setting rate be difficult to when making cooling is constant, especially when the drum length of target is more than 1m, can become uneven tissue at length direction (short transverse in other words as cylinder), the thickness that there is substrate for film deposition becomes uneven problem.In addition, the coarsening of crystal grain also becomes the obstruction of film uniformity.In addition, the problem also having rate of film build fast not.
The present invention completes in view of the foregoing, and its technical problem is, the indium rounding cartridge type sputtering target providing a kind of film thickness distribution good and manufacture method thereof.
For the scheme of dealing with problems
The present inventor carries out effort research in order to solve the problem, find, in indium rounding cartridge type sputtering target, by making the crystal grain footpath miniaturization of target and giving high homogeneity to target length direction, can obtain the sputtering characteristic that film thickness distribution is good.
In existing melting casting, the miniaturization in crystal grain footpath has the limit, and in addition, speed of cooling is also easy produces inequality according to position, therefore, can not obtain this fine and organize uniformly.But the present inventor finds realize this object by carrying out plastic working to indium rounding cartridge type sputtering target under prescribed conditions.
The present invention foundes based on above-mentioned opinion, and be a kind of indium rounding cartridge type target in an aspect, the average crystal grain footpath on sputtered whole surface is 1 ~ 20mm.
In an embodiment of indium rounding cartridge type target involved in the present invention, the crystal grain with linearity crystal boundary is had on sputtered surface, outstanding lower than 0.1mm to vertical line direction of the line segment that this linearity crystal boundary is formed when the adjacent angular of crystal boundary forming crystal grain links with straight line each other, and the linearity region of existence more than 50 μm.
In another embodiment of indium rounding cartridge type target involved in the present invention, synthetic circle of attaching most importance at least partially of described linearity crystal boundary.
In another embodiment of indium rounding cartridge type target involved in the present invention, the Σ value of coincidence crystal boundary is 7.
In another embodiment of indium rounding cartridge type target involved in the present invention, the area ratio with the crystal grain of described linearity crystal boundary is more than 5%.
In another embodiment of indium rounding cartridge type target involved in the present invention, the standard deviation in the average crystal grain footpath on sputtered whole surface is below 6mm.
In another embodiment of indium rounding cartridge type target involved in the present invention, the standard deviation in the average crystal grain footpath at 3 places of length direction central part, an end and the other end is below 0.9mm.
In another embodiment of indium rounding cartridge type target involved in the present invention, to length direction central authorities, an end and the other end, the standard deviation in the average crystal grain footpath measured respectively at the position of the every half-twist of circumferential direction is below 6mm.
The present invention is a kind of manufacture method of indium rounding cartridge type target in another aspect, and it comprises: cast the indium rounding cartridge type target half-finished operation integrated with support tube and radially implement the operation of the plastic working of always rolling shrinkage more than 10% throughout this half-finished whole length direction.
In an embodiment of the manufacture method of indium rounding cartridge type target involved in the present invention, always rolling shrinkage is less than 50%.
In another embodiment of the manufacture method of indium rounding cartridge type target involved in the present invention, comprise: implement plastic working in the mode that the half-finished standard deviation rolling shrinkage circumferentially of described indium rounding cartridge type target is less than 5.
In another embodiment of the manufacture method of indium rounding cartridge type target involved in the present invention, described plastic working is undertaken by any one the above means be selected from the group that is made up of roll compacting, extruding and punching press.
In another embodiment of the manufacture method of indium rounding cartridge type target involved in the present invention, carry out described plastic working with the state of inserting plug in support tube.
Invention effect
According to the present invention, the indium rounding cartridge type sputtering target that film thickness distribution when can provide sputtering in face is good.
Accompanying drawing explanation
Fig. 1 is the example of the crystal structure represented when making the surface be sputtered be easy to observation and take with digital camera for the target (a) obtained by existing casting and target (b) involved in the present invention by etching.
Fig. 2 is the schematic diagram of crystal structure when there is linearity crystal boundary in crystal grain.
Fig. 3 is the schematic diagram of an example of the method representing plastic working.
Embodiment
(1. crystal grain footpath and standard deviation thereof)
The average crystallite particle diameter that indium rounding cartridge type sputtering target involved in the present invention has sputtered whole surface is the feature of below 20mm.Thus, high homogeneity can be guaranteed to the crystal structure of whole target.Average crystal grain footpath is preferably below 18mm, is more preferably below 15mm.When the outside surface by utilizing melting to be cast in the support tube (BT) of round tube type fixes the method manufacture indium rounding cartridge type sputtering target as the indium of target, although the more miniaturization of speed of cooling faster then crystal grain footpath, there is the limit in miniaturization.In addition, be difficult to entirety to cool equably, can produce thick grain at the insufficient position of cooling, be uneven tissue as a whole.But, in the present invention, by utilizing following method to implement plastic working, thus successfully produce the indium rounding cartridge type sputtering target with finer crystal grain and high homogeneity.
But although as long as crystal grain footpath diminishes, then overall homogeneity improves, the stability of film uniformity, sputtering improves, if but certain certain following particle diameter, even if then particle diameter reduces further, the increase effect of consequent film uniformity and sputtering stability also can be reduced.In addition, be made into minimum crystal structure more time-consuming, and cost improves.Therefore, the average crystal grain footpath on sputtered whole surface is preferably more than 1mm, is more preferably more than 1.5mm.
In indium rounding cartridge type sputtering target involved in the present invention, the average crystal grain footpath on sputtered surface measures by the following method.Surperficial with sour slight etching target, make crystal grain boundary be easy to observe after, using the scope of any 100mm × 100mm of the other end (end B) of the scope of any 100mm × 100mm of length direction one end (end A) on the scope of any 100mm × 100mm of the length direction central part on target surface, target surface and the length direction on target surface as a determination object region, counted by the visual number to the crystal grain in each region (N).The crystal grain that trans-regional boundary exists processes as 0.5.In addition, be considered as 0.25 when being positioned at corner to process.
The average crystal grain footpath on whole surface is obtained by measuring following described total 12 regions.In length direction central part, an end, the other end, in the position making determination object region at the every half-twist of circumferential direction, (namely measuring 4 places respectively to each position) measures.Length direction central part refer to one end of length direction is set to 0% length and the other end when being set to the length of 100%, be in the region of the length range of 40 ~ 60%.Equally, an end (end A) refers to the region of the length range being in 0 ~ 20%, and the other end (end B) refers to the region of the length range being in 80 ~ 100%.
By the area (S=10000mm by determination object region 2) average area (s) of the crystal grain in each region is calculated divided by the number (N) of crystal grain.Crystal grain is assumed to be ball and utilizes following formula to calculate average crystal grain footpath (A).
A＝2(s/π) 1/2
Obtaining the average crystal grain footpath in each region thus, therefore, is the average crystal grain footpath on sputtered whole surface by the mean value definition in the average crystal grain footpath in these 12 regions in the present invention.
In addition, if by the standard deviation that the standard deviation definition in the average crystal grain footpath in these 12 regions is sputtered whole surface, then in an embodiment of indium rounding cartridge type sputtering target involved in the present invention, the standard deviation on this whole surface can be made to be below 6mm.In addition, the standard deviation on this whole surface can be made to be preferably below 3mm, be more preferably below 1mm, typical case is 0.1 ~ 5mm.
In addition, Fig. 2 represents the schematic diagram of crystal structure when to there is linearity crystal boundary in crystal grain.As following, target involved in the present invention manufactures owing to implementing plastic working, so there is linearity crystal boundary in common crystal grain, but it yet counts crystal grain as crystal boundary in the present invention.In fig. 2, existence 9 crystal grain are counted out.
In addition, in an embodiment of indium rounding cartridge type sputtering target involved in the present invention, the standard deviation (being called " standard deviation 4 ") in the average crystal grain footpath at 3 places of length direction central part, an end and the other end can be set to below 0.9mm.In addition, this standard deviation can be made to be preferably below 0.8mm, be more preferably below 0.7mm, typical case is 0.1 ~ 0.8mm.The crystal grain footpath of such indium rounding cartridge type sputtering target is higher in the homogeneity of length direction.At this, length direction central part, an end and the other end Shi Ge position, average crystal grain footpath separately makes determination object region at the mean value in the average crystal grain footpath at 4 places that the every half-twist of circumferential direction measures.
In addition, in an embodiment of indium rounding cartridge type sputtering target involved in the present invention, about the everywhere of length direction central authorities, an end, the other end, the standard deviation (being called " standard deviation 1 ", " standard deviation 2 ", " standard deviation 3 ") in the average crystal grain footpath at 4 places measured respectively at the position of the every half-twist of circumferential direction is respectively below 6mm, be preferably below 3mm, be more preferably below 1mm, typical case is 0.1 ~ 3mm.Also even at circumferential direction by crystal grain footpath, thus the advantage that the homogeneity that can obtain sputtered film improves further.
In an embodiment of indium rounding cartridge type sputtering target involved in the present invention, the length of length direction is 500 ~ 4000mm, and typical case is 600 ~ 2500mm, and more typical is 600 ~ 2000mm.
(2. linearity crystal boundary)
In an embodiment of indium rounding cartridge type sputtering target involved in the present invention, the surface sputtered in the acceptance of target has the crystal grain with linearity crystal boundary.In the present invention, " linearity crystal boundary " refers to the outstanding crystal boundary lower than 0.1mm to vertical line direction of the line segment formed when the adjacent angular of the crystal boundary forming crystal grain links with straight line each other.In addition, the thickness of the line segment of evaluation is set to 0.01mm.In addition, straight line refers to the situation of the linearity region of existence more than 50 μm, is not contained in straight line lower than the situations of 50 μm.When being made crystal boundary be easy to observe by etching, although have according to the degree of etching the situation that crystal boundary is etched, and non-linear shape is impaired.Therefore, in the present invention, under these circumstances, the lateral margin of the crystal boundary be etched is defined as the crystal boundary of the crystal grain becoming the object of observation.
In the present invention, " having the crystal grain of linearity crystal boundary " refers in the crystal boundary forming crystal grain, has the crystal grain that more than 1 meets the crystal boundary of the definition of above-mentioned linearity crystal boundary.In the indium rounding cartridge type sputtering target of current goods, crystal grain boundary is roughly curve-like, in contrast, exists in a large number at indium sputtering target parts cathetus shape crystal boundary involved in the present invention.
Linearity crystal boundary must be observed to organize obvious visible mode.Such as, the affected layer being present in target surface is removed by utilizing the etching, electrolytic polishing, sputtering etc. of acid and observed.Observe and undertaken by visual, also can use digital camera, digital microscope, electron microscope etc.Fig. 1 represents that the target parts surface after to sputtering carries out the example with the surface picture of round tube type sputtering target (b) involved in the present invention of linearity crystal boundary and the crystal grain of existing round tube type sputtering target (a) when digital camera is taken.In digital camera photo after sputtering, linearity crystal boundary can be observed in product of the present invention, but not observe in the existing target represented as comparative example.
(3. there is the area ratio of the crystal grain of linearity crystal boundary)
In an embodiment of indium rounding cartridge type sputtering target involved in the present invention, the area ratio with the crystal grain of linearity crystal boundary is more than 5%.By improving the area ratio with the crystal grain of linearity crystal boundary, the effect promoting rate of film build can be obtained.Although its reason is also indefinite, be speculated as the impact of crystal boundary energy etc.If this area ratio is too small, then the lifting effect of rate of film build is less, so be preferably more than 10%, be more preferably more than 20%, more preferably more than 25%, further be preferably more than 30%, further be preferably more than 40% again, and then be further preferably more than 50%, and then be further preferably more than 60% again, especially be preferably more than 70%, such as, can be set to 30% ~ 100%.
In the present invention, the area ratio with the crystal grain of linearity crystal boundary is measured by the following method.Utilize acid to etch indium target, or carry out electrolytic polishing, or sputter, remove the affected layer on surface thus, tissue is easily observed.Afterwards, utilize digital camera etc. to take from face side, by image processing software etc., captured image is obtained to area and the shooting visual field area of the crystallization with linearity tissue.The area ratio with the crystal grain of linearity crystal boundary represents with { (having the crystallization area of linearity tissue)/(shooting visual field area) } × 100 (%).In addition, the size of taking the visual field measures with the area of the crystal grain at least comprising more than 10.
(4. coincidence crystal boundary)
In an embodiment of indium rounding cartridge type sputtering target involved in the present invention, synthetic circle of attaching most importance at least partially (coincidence boundary) of above-mentioned linearity crystal boundary.Coincidence crystal boundary refers to the special crystal boundary that matching is higher geometrically, and compared with only having the material of general crystal boundary (random grain boundary), the material with coincidence crystal boundary has character excellent on chemistry, mechanics mostly.Specifically, coincidence crystal boundary refers to the crystal boundary becoming following relation, that is, when making the adjacent crystallization folk prescription each other clipping crystal grain boundary rotate around crystallographic axis, a part for lattice point periodically consistent with the lattice point of another crystal grain (this lattice point is called coincidence lattice point).Now, original unit's unit cell volume and the ratio of Unit cell volume that newly formed by coincidence lattice point are called Σ value.About coincidence crystal boundary, such as, be recorded in " physics-crystallization of stupalith and interface-" (daily magazine industry newspaper office, several former male writes, 2003,82 pages).
In a typical embodiment of indium rounding cartridge type sputtering target involved in the present invention, linearity crystal boundary is the coincidence crystal boundary of Σ 7.In the present invention, when indium, the crystallization clipping certain crystal boundary be in each other rotate about 85.5 ° (85.5 ° ± 1 °) with < 110 > axle for common rotary axis and the consistent relation in direction time, the Σ value of its crystal boundary is set to 7.The qualification of coincidence crystal boundary Σ 7 can be undertaken by utilizing EBSP (the Electron Backscatter Diffraction Pattern) method of FEEPMA (Field Emission ElectronProbe Micro Analyzer).In usually commercially available FESEM/EBSP device, do not obtain the pattern of coincidence crystal boundary for indium (regular crystal), therefore, specify common rotary axis to be < 110 >, rotation angle is 85.5 °, carries out Σ 7 and to overlap the qualification of crystal boundary.The error at measurment of rotation angle can be different according to each device, but are set to the scope of 85.5 ° ± 1 °.
(5. manufacture method)
Then, the preference of the manufacture method of indium rounding cartridge type sputtering target involved in the present invention is described successively.First, the indium as raw material is melted and is cast in round tube type mold (support tube is through along the length direction concentric circles ground of mold), support tube is used as a part for mold and casts round tube type indium target work in-process.During casting, make well heater be wound in whole mold, mold be heated to 160 DEG C ~ 220 DEG C and carry out air cooling, obtain round tube type target work in-process thus.
If the raw material indium used contains impurity, the efficiency of conversion of the solar cell then made by this raw material reduces, expect that there is high purity due to this reason, such as, can use more than 99.99 quality %, raw material that typical case is the purity of 99.99 quality % ~ 99.9999 quality %.As the material of supporting plate, arbitrary material well known to the skilled person can be adopted, include, for example stainless steel, titanium, copper, from the aspect that the solid solution to indium is less, be preferably stainless steel and titanium.
Then, radially plastic working is implemented to the round tube type target work in-process obtained by casting.Oversize particle is more substantially for casting target, and uneven, but by carrying out plastic working and recrystallizing (indium can recrystallize at normal temperatures fully) and generate fine crystal structure.Plastic working can be carries out either party of roll compacting, extruding, punching press etc. in radial direction, in addition, can be cold rolling also can be hot rolling.If plastic working always to roll shrinkage too low, then the miniaturization of crystal structure can not fully be in progress, so the mode preferably reaching more than 10% always to roll shrinkage is implemented, is more preferably the mode reaching more than 13% and implements.On the other hand, if it is too high always to roll shrinkage, then the thickness for obtaining the cast body needed for products thickness is thickening, and the effect of miniaturization also reduces, and therefore, the mode preferably reaching less than 35% always to roll shrinkage is implemented, and the mode being more preferably to reach less than 33% is implemented.
At this, roll shrinkage (r:%) with following formula: r=(h 2-h 1)/h 2× 100 (in formula, h 2for the radial thickness of the target before plastic working, h 1radial thickness for the target after plastic working) definition.In addition, always roll shrinkage and be at one end set to the mean value rolling shrinkage at 4 places measured at the every half-twist of circumferential direction in portion.
In addition, in order to improve the homogeneity in crystal grain footpath circumferentially, the mode that plastic working preferably reaches less than 5 with the half-finished standard deviation rolling shrinkage circumferentially of above-mentioned indium rounding cartridge type target is implemented, the mode being more preferably to reach less than 3 is implemented, and then preferably implements in the mode reaching less than 1.The standard deviation rolling shrinkage circumferentially calculates by the following method.Measure the target thickness after target thickness and plastic working after the casting at above-mentioned 4 places, obtain at each position and roll shrinkage, and calculate the standard deviation rolling shrinkage at 4 places.
Below enumerate and use the example of punching press as an example.
Method can be listed below: the fixing round tube type target work in-process terminating casting make it not move, and vertically carry out punching press to these round tube type target work in-process relative to seat surface.
At this, in order to make uniform crystal particles at the length direction of target and circumferential direction respectively, preferably making to roll shrinkage at length direction and circumferentially identical, and then, can carry out rolling contracting to eliminate the mode rolled contracting and roll the seam between contracting.
In addition, be desirably in when rolling contracting, make to have in the indeformable mode of the drum of target and insert inside with the internal diameter of support tube with the plug of the external diameter of degree.As the material of plug, as long as be the material of the hardness with the degree of not being out of shape because of plus-pressure during punching press, be just not particularly limited, such as, can enumerate stainless steel, cast iron, from the view point of preventing rust etc. to be infected with, being preferably stainless steel.
Such as in figure 3, adopt and utilize the pedestal (101) of mounting round tube type target work in-process (100) and the fixing method of two supporting stations (102) before and after turning direction can not be located in the upper mode of rotating of pedestal (101) with target work in-process (100).In figure 3, supporting station (102) be plane with the contact surface of round tube type target work in-process (100), but be not limited to this, such as, the surface shape of itself and round tube type target work in-process (100) also can be made to coincide and arc-shaped bend.
In addition, in roll compacting, as long as use multiple roller clip round tube type indium target work in-process in radial direction and make it with the central shaft of cylinder for turning axle rotates, apply pressure and roll compacting rolls shrinkage to what specify simultaneously.The homogeneity of circumferential direction crystal grain can be kept like this.Or, it also can not be made to rotate and carry out roll compacting indium target using the half-finished length direction of indium target as roll compacting direction.In this case, identical with punching press, as long as make target rotate a little when each roll compacting.In extrusion processing, as long as make indium target by having the pipe of desired diameter.Now, pipe also can have tapering.In addition, expect suitably to adjust extrusion speed.
The thickness of the radial direction of the indium after plastic working is not particularly limited, and suitably set according to the sputter equipment used or film forming duration of service etc., be generally about 5 ~ 20mm, typical case is about 8 ~ 15mm.
The indium rounding cartridge type sputtering target obtained like this can be suitable as the sputtering target that CIGS thin-film solar cells light absorbing zone makes.
Embodiment
Represent embodiments of the invention in the lump with comparative example below, these embodiments provide to better understand the present invention and advantage thereof, are not intended to limit invention.
In following embodiment and comparative example, the SUS304 support tube of the size of use length 640mm, internal diameter 125mm, external diameter 133mm, manufactures the indium target of target length 600mm, internal diameter 133mm, external diameter 151mm size.
< embodiment 1 >
Melt the indium as raw material, and be cast in round tube type mold (support tube is through along the length direction concentric circles ground of mold), support tube is used as a part for mold and casts indium target work in-process.The material of mold is set to SUS304.The indium of raw material uses the raw material that purity is 4N.During casting, be wound in by well heater on whole mold, heated mold to 180 DEG C in advance, cooling adopts air cooling.The thickness of the half-finished radial direction of indium target after casting is set to 14mm (target external diameter is 161mm).
This casting target is colded pressing in the mode described in Fig. 3.In a punching press, in order to carry out punching press to upper surface and these two faces of lower surface, often rotating 5 ° and carry out punching press and make it rotate 180 °, implement plastic working to whole.In addition, in support tube indeformable mode, the plug of SUS304 is inserted in support tube.On average rolling contracting amount is the one-sided 1.5mm contracting amount of on average rolling of upper surface side and the lower face side (add up to 3.0mm), and always to roll shrinkage be 10.6%.The mean value rolling shrinkage that at one end portion (end A) measures in 4 places that circumferentially every half-twist measures is referred in this said shrinkage of always rolling.In addition, the standard deviation circumferentially rolling shrinkage is shown in table 1.Obtained target is lathed and is processed into above-mentioned size, make round tube type indium target.Cold pressing and refer to punching press under normal temperature condition.
< embodiment 2 >
With on average roll contracting amount be one-sided 2mm, always roll shrinkage be 14.3% mode carry out punching press, make round tube type indium target similarly to Example 1 in addition.
< embodiment 3 >
With on average roll contracting amount be one-sided 2.6mm, always roll shrinkage be 18.4% mode carry out punching press, make round tube type indium target similarly to Example 1 in addition.
< embodiment 4 >
With on average roll contracting amount be one-sided 3.0mm, always roll shrinkage be 21.5% mode carry out punching press, make round tube type indium target similarly to Example 1 in addition.
< embodiment 5 >
With on average roll contracting amount be one-sided 3.9mm, always roll shrinkage be 27.6% mode carry out punching press, make round tube type indium target similarly to Example 1 in addition.
< embodiment 6 >
With on average roll contracting amount be one-sided 4.4mm, always roll shrinkage be 31.7% mode carry out punching press, make round tube type indium target similarly to Example 1 in addition.
< embodiment 7 >
With on average roll contracting amount be one-sided 7mm, always roll shrinkage be 50.0% mode carry out punching press, make round tube type indium target similarly to Example 1 in addition.
< embodiment 8 >
In embodiment 8, note making always to roll shrinkage constant at circumferential direction, on one side with on average roll contracting amount be one-sided 2.5mm, always roll shrinkage be 17.8% mode under the condition of 100 DEG C, carry out punching press, making round tube type indium target similarly to Example 1 in addition.
< embodiment 9 >
In embodiment 9, note making always to roll shrinkage constant at circumferential direction, on one side with on average roll contracting amount be one-sided 2.6mm, always roll shrinkage be 18.2% mode under the condition of 100 DEG C, carry out roll compacting, making round tube type indium target similarly to Example 1 in addition.
< embodiment 10 >
In embodiment 10, note making always to roll shrinkage constant in circumferential direction, on one side with on average roll contracting amount be one-sided 2.6mm, always roll shrinkage be 18.3% mode under the condition of 25 DEG C, carry out roll compacting, making round tube type indium target similarly to Example 1 in addition.
< embodiment 11 >
In embodiment 11, note making always to roll shrinkage constant in circumferential direction, on one side with on average roll contracting amount be one-sided 2.5mm, always roll shrinkage be 17.8% mode under the condition of 25 DEG C, carry out extrusion processing, making round tube type indium target similarly to Example 1 in addition.
< comparative example 1 >
Identical with embodiment 1 to manufacture casting target, but do not carry out plastic working and lathe and be machined to said products size, make round tube type indium target.
< comparative example 2 >
With on average roll contracting amount be one-sided 0.3mm, always roll shrinkage be 2.2% mode carry out punching press, make round tube type indium target similarly to Example 1 in addition.
< comparative example 3 >
With on average roll contracting amount be one-sided 0.5mm, always roll shrinkage be 3.7% mode carry out punching press, make round tube type indium target similarly to Example 1 in addition.
< comparative example 4 >
With on average roll contracting amount be one-sided 1.1mm, always roll shrinkage be 7.7% mode carry out punching press, make round tube type indium target similarly to Example 1 in addition.
(average crystal grain footpath)
According to above-mentioned measuring method, the indium target obtained is obtained respectively to average crystal grain footpath and the standard deviation on whole surface in embodiment and comparative example from above-mentioned 12 regions.In addition, in length direction central authorities, end A, end B, every 90 °, average crystal grain footpath is measured at circumferential direction respectively, also calculate its standard deviation (being called " standard deviation 1 ", " standard deviation 2 ", " standard deviation 3 ").And then, also calculate the standard deviation (being called " standard deviation 4 ") in average crystal grain footpath of length direction central authorities, end A and end B.Show the result in table 2.
[table 1]
[table 2-1]
[table 2-2]
(there is the area ratio of the crystal grain of linearity crystal boundary)
In addition, to the indium target obtained in embodiment and comparative example, after etching according to aforesaid method hydrochloric acid respectively, utilize digital camera to take, and use image processing software (Olympus society manufactures analySISFIVE) to measure the area ratio with the crystal grain of linearity crystal boundary.Show the result in table 3.
(coincidence crystal boundary)
In addition, to each embodiment and comparative example, by using the EBSP method of FE-EPMA (Jeol Ltd. JXA8500F) to carry out the mensuration of crystal orientation, and judge that the coincidence crystal boundary of crystal grain boundary is whether as Σ 7 according to aforesaid method.In addition, the TSLOIM Analysis that the software application TexSem Laboratories company analyzed manufactures.Show the result in table 3.
[table 3]
(sputtering characteristic)
The indium target obtained in embodiment and comparative example is sputtered, respectively at position (the amount to 3 places) placement substrate corresponding with length direction central authorities and both ends, and measures its sputtering thickness.Specifically, sputter with following condition, and calculate the thickness of obtained film according to the weight of the substrate before and after sputtering.In addition, the mean value based on the thickness at 3 places calculates rate of film build.Show the result in table 4.
Sputtering condition is as follows.
Sputter gas: argon gas
Sputtering pressure: 0.5Pa
Sputter gas flow: 50SCCM
Sputter temperature: R.T. (not heating)
Drop into Sputtering power density: 1.3W/cm 2
(power density is the every 1cm to target surface 2input power)
Substrate: the Eagle2000 that Corning company manufactures, inch × 0.7mmt
Pre-sputtering: carry out 1h with above-mentioned condition
[table 4]
(investigation)
According to the above results, the sputtering target involved by known the application of the invention sputters, can in face film forming equably.In addition, by using the sputtering target being formed with linearity crystal boundary, rate of film build also improves.
Comparative example 1 is the example not carrying out punching press, and known coarse grains and standard deviation are also large, create inequality at target length direction.In addition, the distribution of thickness is also uneven.
Although comparative example 2 ~ 4 has carried out punching press, less owing to always rolling shrinkage, so the still thick and standard deviation of crystal grain is also large, produce uneven at target length direction.In addition, the distribution of thickness is also uneven.
Description of reference numerals
100: round tube type target work in-process
101: pedestal
102: supporting station
103: indium
104: support tube
105: plug

Claims (13)

1. an indium rounding cartridge type target, the average crystal grain footpath on sputtered whole surface is 1 ~ 20mm.
2. indium rounding cartridge type target as claimed in claim 1, wherein, the crystal grain with linearity crystal boundary is had on sputtered surface, outstanding lower than 0.1mm to vertical line direction of the line segment that this linearity crystal boundary is formed when the adjacent angular of crystal boundary forming crystal grain links with straight line each other, and the linearity region of existence more than 50 μm.
3. indium rounding cartridge type target as claimed in claim 2, wherein, synthetic circle of attaching most importance at least partially of described linearity crystal boundary.
4. indium rounding cartridge type target as claimed in claim 3, wherein, the Σ value of coincidence crystal boundary is 7.
5. the indium rounding cartridge type target according to any one of claim 2 ~ 4, wherein, the area ratio with the crystal grain of described linearity crystal boundary is more than 5%.
6. the indium rounding cartridge type target according to any one of Claims 1 to 5, wherein, the standard deviation in the average crystal grain footpath on sputtered whole surface is below 6mm.
7. the indium rounding cartridge type target according to any one of claim 1 ~ 6, wherein, the standard deviation in the average crystal grain footpath at 3 places of length direction central part, an end and the other end is below 0.9mm.
8. the indium rounding cartridge type target according to any one of claim 1 ~ 7, wherein, to length direction central authorities, an end and the other end, the standard deviation in the average crystal grain footpath measured respectively at the position of the every half-twist of circumferential direction is below 6mm.
9. a manufacture method for indium rounding cartridge type target, it comprises: cast the indium rounding cartridge type target half-finished operation integrated with support tube and radially implement the operation of the plastic working of always rolling shrinkage more than 10% throughout this half-finished whole length direction.
10. the manufacture method of indium rounding cartridge type target as claimed in claim 9, wherein, always rolling shrinkage is less than 50%.
The manufacture method of 11. indium rounding cartridge type targets as described in claim 9 or 10, it comprises: implement plastic working in the mode that the half-finished standard deviation rolling shrinkage circumferentially of described indium rounding cartridge type target is less than 5.
The manufacture method of 12. indium rounding cartridge type targets according to any one of claim 9 ~ 11, wherein, described plastic working is undertaken by any one the above means be selected from the group that is made up of roll compacting, extruding and punching press.
The manufacture method of 13. indium rounding cartridge type targets according to any one of claim 9 ~ 12, wherein, carries out described plastic working with the state of inserting plug in support tube.
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